2,6-二氯-4-硝基苯胺 → 3-(3,5-DICHLORO-4-METHYLBENZOYL)PROPIONIC ACID

HRID 1562

反应方程式

HRID 1562 反应方程式
[CH3:1][C:2]1[CH:14]=[CH:13][C:5]([C:6]([CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[O:7])=[CH:4][CH:3]=1.[Cl-:15].[Al+3].[Cl-:17].[Cl-].ClCl>C(Cl)Cl>[Cl:15][C:3]1[CH:4]=[C:5]([CH:13]=[C:14]([Cl:17])[C:2]=1[CH3:1])[C:6]([CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[O:7]

参与物

5

反应物 3

HCID 245262,6-二氯-4-硝基苯胺HCID 2441623-(4-甲基苯甲酰)丙酸HCID 6451240三氯化铝

产物 1

HCID 125335863-(3,5-DICHLORO-4-METHYLBENZOYL)PROPIONIC ACID收率 44.2%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

To a mixture of 3-(4-methylbenzoyl)propionic acid (7.5 g) and methylene chloride (250 ml) was added slowly portionwise aluminum chloride (15 g) at 0° C. After the addition was completed chlorine gas was bubbled in slowly at 0° C. After 6 hours the reaction mixture was poured into a mixture of hydrochloric acid and ice and extracted with methylene chloride (3×150 ml), the combined organic layers were washed with water, dried and evaporated under vacuum yielding 3-(3,5-dichloro-4-methylbenzoyl)propionic acid as a yellow solid (4.5 g).

后处理

  1. additionAfter the addition
  2. customwas bubbled in slowly at 0° C
  3. additionAfter 6 hours the reaction mixture was poured into a mixture of hydrochloric acid and ice
  4. extractionextracted with methylene chloride (3×150 ml)
  5. washthe combined organic layers were washed with water
  6. customdried
  7. customevaporated under vacuum

来源与证据

ORD记录
ord-6293fd2e9db947d781cf392334ab42c8
来源数据集
uspto-grants-1998_03
专利号
US05726176

关联笔记

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